| 引用本文: | 陈仕云,杨士伟,何勇,韩冬,吴宗好,高永好.盐酸文拉法辛光降解杂质的合成[J].中国现代应用药学,2021,38(3):266-268. |
| CHEN Shiyun,YANG Shiwei,HE Yong,HAN Dong,WU Zonghao,GAO Yonghao.Synthesis of Photodegradation Impurities from Venlafaxine Hydrochloride[J].Chin J Mod Appl Pharm(中国现代应用药学),2021,38(3):266-268. |
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| 摘要: |
| 目的 合成盐酸文拉法辛的光降解杂质1-[2-（二甲胺基）-1-（4-甲氧苯基）乙烯基]-1-环己烷（杂质I），加强对二环类非典型抗抑郁药盐酸文拉法辛原料药的质量控制。方法 对甲氧基苯乙腈与环己酮经缩合反应，LiAlH4还原反应，甲酸/甲醛双甲基化反应得到光降解杂质I。结果 杂质I的结构经1H-NMR、13C-NMR和MS确证，纯度经HPLC检测>99.0%。结论 杂质I可作为盐酸文拉法辛原料药质量控制的杂质对照品。 |
| 关键词: 抗抑郁 盐酸文拉法辛 光降解杂质 有机合成 |
| DOI：10.13748/j.cnki.issn1007-7693.2021.03.002 |
| 分类号:R914.5 |
| 基金项目:“重大新药创制”国家科技重大专项（2017ZX09201003） |
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| Synthesis of Photodegradation Impurities from Venlafaxine Hydrochloride |
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CHEN Shiyun1, YANG Shiwei2, HE Yong2, HAN Dong2, WU Zonghao2, GAO Yonghao2
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1.Analytical & Testing Center, Hefei University, Hefei 230601, China;2.Hefei Huafang Pharmaceutical Science & Technology Co., Ltd., Hefei 230088, China
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| Abstract: |
| OBJECTIVE To perform the quality control of the bicyclic atypical antidepressant venlafaxine hydrochloride bulk medicine, the venlafaxine hydrochloride photodegradable impurities I[2-cyclohexylidene-2-(4-methoxyphenyl)-N,Ndimethylethanamine] was prepared. METHODS Through condensation reaction of p-methoxyphenylacetonitrile and cyclohexanone, LiAlH4 reduction reaction, formic acid/formaldehyde double methylation reaction, photodegradable impurities I was obtained. RESULTS The structures of impurities I were confirmed by 1H-NMR, 13C-NMR, MS, and the HPLC indicated that the purity of product was higher than 99.0%. CONCLUSION The impurities I can be used as impurity reference for quality control of venlafaxine hydrochloride active pharmaceutical ingredient. |
| Key words: antidepressant venlafaxine hydrochloride photodegradable impurities organic synthesis |
